Construction and Building Materials xxx (2011) xxx–xxx

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Construction and Building Materials

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Microstructural characterisation and physical properties of cured thermally

activated clay-lime blends
Y. Mleza, M. Hajjaji ⇑
Laboratoire de Physico-chimie des Matériaux et Environnement, Unité Associée au CNRST (URAC 20), Département de Chimie, Faculté des Sciences Semlalia,
Université Cadi Ayyad, B.P. 2390, Marrakech, Morocco

a r t i c l e i n f o a b s t r a c t

Article history: The microstructure of cured mixes consisting of thermally activated clay and lime (up to 20 wt.%) was
Received 8 April 2010 investigated using X-ray diffraction, Fourier transform infrared spectrometry and scanning electron
Received in revised form 30 April 2011 microscopy. Additionally, changes of bending strength, density and water absorption against curing time
Accepted 13 June 2011
and lime addition were followed. The results showed that calcium silicate hydrate (C–S–H) and monocal-
Available online xxxx
cium aluminate decahydrite (CAH10) together with calcite formed. The occurrence of C–S–H and CAH10
involved chemical reactions between hydrated lime, micaceous species and quartz, and metakaolin
Keywords:
respectively. The development of the cementitious products, favoured by the increase of lime admixture
Heated clay
Lime
and ageing time, contributed to the increase of the mechanical resistance, but its impact on the remaining
Curing physical properties was somewhat irregular. Regarding water absorption, it was found that the kinetic
Microstructure of the process obeyed a pseudo-first order equation and the constant was in the range
Physical properties (10.6–16.2)  10 2 min 1.
Ó 2011 Elsevier Ltd. All rights reserved.

1. Introduction chemical stability and physical properties of thermally activated

Raw clays together with lime have been widely used for con-
struction of buildings and monuments [1]. Phyllosilicates (the
main constituents of clays) are able to react with lime to give to
cementitious products. The pozzolanic activity of these minerals
depends on their mineralogical nature, chemical composition and
particles size as well as on the operating conditions (ageing dura-
tion, temperature and pH) [2,3].
Ordinary cements are obviously good cementing materials, but
their production requires considerable energy and generates huge
quantities of carbon dioxide [4,5]. Therefore, many studies have
been undertaken to reduce their content in mortars and concretes,
and even to find substitutes. In this connection, it is reported that
metakaolin, a heated kaolinite derived phase, has high pozzolanic
activity and may be to a certain extent used as a substitute for or-
dinary cements [6–8]. In the presence of hydrated lime, metakaolin
could lead, at ordinary temperature, to cementitious products such
as calcium silicate hydrate (C–S–H), stratlingite (C2ASH8) and
C4AH13 [9–11].
While the pozzolanic activity of heat-treated kaolinite has been
investigated [12–14], little attention has been paid to the study of
the cementing behavior of thermally activated mixes of clay min-
erals or naturally occurring clays [15]. The improvement of the
⇑ Corresponding author. Fax: +212 524 43 74 08.
E-mail address: hajjaji@ucam.ac.ma (M. Hajjaji).
clay-based cements may be of great interest for repairing historical
buildings. Mortars consisting of local natural pozzolanic materials
could be compatible with the original materials of local building
monuments [16]. Moreover, addition of natural pozzolans to
lime-releasing cements, such as Portland cement, may improve
the resistance to corrosive sulphate and chlorine solutions, reduces
the susceptibility to expansion due to alkali–silica reactions, and
diminishes the heat evolution during cement hydration [17,18].
The aim of this work was to investigate the microstructure of
cured blends consisting of thermally activated clay and lime, and
to follow changes of some physical properties against lime addition
and curing duration.
2. Materials and experimental procedures
2.1. Materials
The clay was from the valley of Ourika (High-Atlas Mountain, Morocco). It is a
non-calcareous red clay composed of kaolinite (34 wt.%), mica/illite (32 wt.%),
quartz (21 wt.%) and hematite (6 wt.%). Its chemical composition is reported in Ta-
ble 1. To be used, the raw clay was gently grounded and heated at 600 °C for 2 h.
Under such heating conditions, the dehydroxylation of kaolinite was complete.
The grain size distribution of the heated clay is shown in Fig. 1. Because of heating,
kaolinite disappeared, whereas micaceous species, quartz and hematite were unaf-
fected (Fig. 2).
The lime was a commercial local material used for bleaching external shelter
walls. It was grounded and its grain size distribution was determined (Fig. 1). It con-
sisted almost of portlandite (Fig. 2). The quantity of oxides associated to the calcium
oxide, forming the material used, was about 10 wt.% (Table 1).

0950-0618/$ - see front matter Ó 2011 Elsevier Ltd. All rights reserved.
doi:10.1016/j.conbuildmat.2011.06.014

Please cite this article in press as: Mleza Y, Hajjaji M. Microstructural characterisation and physical properties of cured thermally activated clay-lime
blends. Constr Build Mater (2011), doi:10.1016/j.conbuildmat.2011.06.014
2 Y. Mleza, M. Hajjaji / Construction and Building Materials xxx (2011) xxx–xxx

Table 1 purpose, thin pastilles consisting of 0.02 g of cured samples and 0.48 g of KBr
Chemical compositions of thermally activated clay (TAC) and lime. were prepared. SEM examinations were conducted on carbon coated fractured
surfaces by a JEOL JMS 5500 microscope equipped with LINK-OXFORD XLII EDAX
SiO2 Al2O3 Fe2O3 MgO CaO Na2O K2O Lia system.
TAC 43.2 23.3 9.1 5.1 1 0.8 5.7 6.8 The flexural strength (r) of cured test-pieces was evaluated according to the
Lime 5.8 1.9 0.2 2.1 89.3 Trb 0.1 ndc relation: r = 3/2[(F  L)/(b  h2)], where F (in N) is the maximum load. L = 2.8 cm,
7.1 < h < 7.2 mm and 10.2 < b < 10.4 mm. Density (d) of cured samples was deter-
a
Loss on ignition. mined by pycnometry using edible oil (d = 0.918) as a solvent. The weight of ab-
b
Traces. sorbed water was followed as a function of time. In this case, cured samples were
c
Not determined. placed on a water immersed sponge. Measurements of pH were realized on suspen-
sions composed of 1 g of cured samples and 4 ml of distilled water.

100 Lime Heated raw clay 3. Results and discussion

3.1. Phases identification

80
The analysis of X-ray diffraction patterns of cured samples
(Fig. 3) showed that: (i) quartz and micaceous species (original
% Retained

60
40
20
0 lime-rich samples and lengthy curing periods (Fig. 3b). Apparently,
0.0 0.1 0.2 0.3
Grain size (mm)
Fig. 1. Grain size distribution of the used materials.
2.2. Experimental procedures
Homogenised blends of powdered samples of the dry heated clay and lime (up
to 20 wt.%) were mixed with an optimum quantity of distilled water (water/
blend = 40 wt.%) and worked for 10 min to obtain a consistent paste. Prismatic sam-
ples (10  7.2  5 mm3), which were convenient for mechanical tests, were shaped
from the fresh paste by manual pressing, using a stainless steel mould. The as-pre-
pared bars were cured for different times (until 28 days) at 22 ± 2 °C in a humid
(100% moisture) partially hermetic plastic box.
Microstructural change of the aged test-pieces was investigated by X-ray dif-
fraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and scanning
electron microscopy (SEM). The XRD analyses were carried out on hand-
grounded samples, using a Philips X’Pert MPD diffractometer equipped with a
copper anticathode (k = 1.5418 Å). The FT-IR spectra were recorded by a Perkin
Elmer spectrophotometer functioning in the range 4000 and 400 cm 1. For this
minerals) were encountered in whole cured test-pieces, but their
amounts varied with lime addition and curing duration. As can
be seen in Fig. 4, the amount of micaceous species considerably de-
creased up to about 7 wt.% lime, when that of quartz experienced a
slight and almost steady decline; (ii) lime admixture resulted in
the occurrence and intensification of portlandite reflections; (iii)
broad and less intense reflections particularly manifested for
0.4 0.5
they are attributed to monocalcium aluminate decahydrite –
CAH10 – (JPDF 47-1882); and (iv) the peak at 3.03 Å (2h = 29.5°),
which could be assigned, among others, to the main X-ray reflec-
tion of calcite, intensified as the lime content exceeded 7 wt.%.
However, its intensity exhibited a maximum for <7 wt.% lime
(Fig. 5).
FT-IR spectra of cured mixes (Fig. 6) exhibited bands relevant to
calcite (2524, 1458.9, 873, 712 cm 1) [19], quartz (799, 778,
695 cm 1) [20] and water hydration (3472, 1638 cm 1) [20]. The
presence of mica/illite was revealed by the band at about
3627 cm 1, corresponding to Al–Al–OH stretching vibration [21].
In agreement with the XRD results, the structure of micaceous spe-
cies did not destabilized by heating. However, as a result of lime
additions, profiles and intensities of bands relevant to mica/illite
or quartz were altered, apparently because of their implication in
chemical reactions. The pozzolanic reactions at room temperature
of illite and quartz with lime were also reported by Ninov and Don-
chev [22] and Millogo et al. [23] respectively. Opposing to XRD, IR

300
P

P P
C
P
200 P
L PP
L P
Intensity

b
Q Q
Q Q
100 Q
Q
Q Q Q
H H Q H
M Q Q
M M H Q
M
M MM
a
0
10 20 30 40 50 60 70
2Θ °

Fig. 2. X-ray diffraction patterns of the thermally activated clay (a) and lime (b) M: Micaceous species; Q: Quartz; H: Hematite; P: Portlandite; L: Quicklime; C: Calcite.

Please cite this article in press as: Mleza Y, Hajjaji M. Microstructural characterisation and physical properties of cured thermally activated clay-lime
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 Y. Mleza, M. Hajjaji / Construction and Building Materials xxx (2011) xxx–xxx 3

2 6 8 16 wt.% lime (a)

600
Q

M Q
Q
Q P Q Q
Q Q P P,Q Q
M M Q P
P Q P
M
400

Intensity

200
H
M M M,H
H
M M

10 20 30 40 50 60 70
2Θ °

2 6 8 16 wt.% lime
(b)
Q M Q
H Q
20 Lime content: 16 wt.% ; Curing time: 28 days 500 Q P Q Q
MQ
Intensity

M Q
CAH10 Q
Intensity

P Q
M P P

CAH10 400

CAH10
10
300

200
M H H
M H,M
0 M
5 15
2Θ ° 20
10 M
100
10 20 30 40 50 60 70
2Θ °

Fig. 3. Representative X-ray diffractograms of thermally activated clay-lime samples cured 7 (a) and 28 (b) days. M: Micaceous species; Q: Quartz; H: Hematite; P:
Portlandite; CAH10: Monocalcium aluminate decahydrite.

0.426 nm reflection of quartz

Intensity of the IR band at 1439 cm-1

Relative X-ray intensity of 0.303 nm

0.448 nm reflection of micaceous species 1.2

1.6
1.0
Relative X-ray intensity

1.4
0.8
of calcite
reflection

0.8
1.2

0.4
1.0

0.6 0.8 0.0

0 4 8 12 16
Lime content (wt.%)

Fig. 5. Evolution of the intensity of the X-ray 0.303 nm reflection and the
0 4 8 12 16 1439 cm 1 IR band of calcite versus lime addition.
Lime content (wt.%)

Fig. 4. Variation of the amounts of mica/illite and quartz against lime addition.
Curing time: 28 days. which main characteristic bands partly overlapped with those of
water (3432 cm 1) and micaceous species (3627 cm 1). The dou-
analyses allowed to detect calcite even in lime poor samples, i.e. blet occurring at about 2363 and 2337 cm 1 is attributed to
2 wt.% lime mix. dissolved carbon dioxide of atmosphere. The gas dissolution did
The broadening and the asymmetric shape of the band at about not happen for 2 wt.% lime cured samples, but it intensively and
1439 cm 1 are presumably due to the presence of portlandite [24], arbitrary took place in lime rich mixes.

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4 Y. Mleza, M. Hajjaji / Construction and Building Materials xxx (2011) xxx–xxx

(a) 2; 6; 8; 12; 16; 20 wt.%

2.0

1023

693.3
1444.4

798.4
1.5

876.5
713.5
Absorbance (%)

478.3
1795.4
1642.1
1.0

2356.6

773.3
556.4
3447.1
3643.8

2338.3

1886
0.5

2510
0.0
4000 3500 3000 2500 2000 1500 1000 500
Wavenumber (cm-1)

(b) 2.0 2; 6; 8; 12; 16; 20 wt.%

1024.9

877.4
1449.2

481.2
777.2
1.5

564
799.3
Absorbance (%)

717.4
1632.4
3467.5

1.0
3627.4

692.3
2364.3

2335.4
2513.7

0.5

0.0
4000 3500 3000 2500 2000 1500 1000 500
Wavenumber (cm-1)

Fig. 6. IR spectra of mixes cured 7 (a) and 28 (b) days.

The change of the relative intensity of the X-ray reflection at
3.03 Å, attributable to calcite, versus lime addition showed a max-
imum for <7 wt.% (Fig. 5). As a matter of fact, the amount of calcite
should continuously increase as revealed by the IR results (Fig. 5).
Thus, it is believed that the considered peak is shared with the in-
tense reflection of calcium silicate hydrate (C–S–H), which is com-
monly encountered in such chemical environment [25,26]. The less
intense X-ray reflections (2.79; 1.82, 1.66 Å) [27] related to this
compound were presumably hidden. As far as the C–S–H presence
is concerned, it may noted that because of the occurrence of the
complex IR band at around 1024 cm 1 relevant to Si–O–Si stretch-
ing vibrations of micaceous species and some clay minerals deriv-
ing species [20], the characteristic and intense band of C–S–H
(about 970 cm 1) [24] could not be resolved.
3.2. Microstructure examination and physical properties
By referring to the microstructure of lime-free samples (Fig. 7a),
lime additions as low as 2 wt.% resulted in the formation of coarse
and pseudo-spherical particles as well as a less segregated micro-
structure (Fig. 7b). For moderate lime additions (6–8 wt.%), linkage
between particles was apparently enhanced and micaceous parti-
cles exhibited irregular edges and pointed extremities (Fig. 7c).
Regarding the latter observation, it is believed that because of
the increase of pH due to lime additions (Fig. 8), micaceous parti-
cles were subjected to partial etching. On the other hand, in view
of the above results, bonds between clay particles could be related
to the formation of C–S–H, considered as a cementitious product.
However, it is not excluded that particles bonding in 2 wt.% sam-
ples was chiefly accomplished by flocculation and agglomeration,
which happened as a result of the adsorption of calcium cations
on clay particles [28]. This postulate is based on the fact that these
samples were disaggregated upon water absorption.
The microstructure of lime-rich samples was essentially con-
sisted of dense pseudo-tangled filaments (Fig. 7d). Such filamen-
tous feature was also observed around coarse particles of quartz
(Fig. 7e). The occurrence of this kind of microstructure concurred
with the development of CAH10. In this case, scarce polygonal

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 Y. Mleza, M. Hajjaji / Construction and Building Materials xxx (2011) xxx–xxx 5

(a) (d)

(b) (e)

(c)
(f)

Fig. 7. SEM micrographs of lime free sample (a) and mixes cured 28 days ((b): 2; (c): 6; (d), (e) and (f): 20 wt.% lime).

12 28 21 14 7 days of curing
precipitates, such as presented in Fig. 7f, were encountered. Be-
cause of their tiny size, the precipitates could not be identified
by SEM. A careful examination showed that the adjacent areas to
11
these precipitates were exempt of filaments, apparently, because
of their coalescence happened at the expense of the filamentous
product.
pH

The cementation of clay particles due to the increase of curing

10
duration and lime content induced samples strengthening. The
maximum of bending strength (4 MPa) was observed for long age-
ing time and lime rich samples (Table 2). The cementation process
also influenced mixes density (Table 3). However, as compared
9
with the bending strength, the maximum of density (3.1) was
0 5 10 15 20 reached after 21 days of curing. In view of these results, it may
be stated that the occurring changes of microstructure, due to lime
Lime (wt.%)
admixture and ageing, did not have similar impacts on the consid-
Fig. 8. Variation of pH of cured mixes versus lime addition. ered properties.

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6 Y. Mleza, M. Hajjaji / Construction and Building Materials xxx (2011) xxx–xxx

Table 2 and Qe are quantities of water absorbed at t instant and equilib-

Bending strength (MPa) of the studied thermally activated clay-lime blends. rium respectively; k is the kinetic constant which values varied
Curing time (days) Lime content (wt.%) in the range (10.6–16.2)  10 2 min 1 for 28 days of curing. As T
2 6 8 12 16 20 was constant, the variation of k is related to the microstructure
change.
7 0.34 0.96 1.07 1.11 0.59 0.95
14 0.36 1.30 1.51 3.71 2.45 2.57
21 0.37 2.03 2.33 2.58 2.27 3.28 3.3. Phases formation mechanism
28 0.41 2.20 2.84 2.90 3.16 4.10
The partial vanishing of micaceous species and quartz observed
for <7 wt.% lime additions (Fig. 4) and the concomitant formation
of C–S–H led to think that a part of the cementitious product de-
Table 3 rived from the reaction between the considered minerals and hy-
Density of the cured thermally activated clay- lime mixes.
drated lime. As a matter of fact, such chemical transformation
Curing time (days) Lime content (wt.%) depended essentially on the availability of fine quartz [23] as well
2 6 8 12 16 20 as silica located at edges of tetrahedral sheets of mica/illite. The
7 2.62 2.69 2.44 2.42 2.39 2.39
contribution of silica of metakaolin, deriving from heated kaolinite,
14 2.68 2.64 2.54 3.02 2.85 2.80 for forming C–S–H is not excluded. In this connection, it may be
21 3.13 2.86 3.09 3.06 3.18 2.91 mentioned that the required Ca/Si molar ratio for the formation
28 2.85 2.95 2.76 2.69 2.64 2.60 of C–S–H should be in the range 0.7–2.3 [27], whereas the actual
ratios did not exceed 0.5. Therefore, only highly reactive silica (fine
quartz, border bounded silica and metakaolin silica) seems to be
involved in C–S–H formation.
Table 4
As lime addition exceeded 7 wt.%, the amount of portlandite
Water absorption (wt.%) of the studied cured blends.
and calcite increased and pH became almost constant (Fig. 8).
Curing time (days) Lime content (wt.%) Apparently, because of the depletion of the potentially reactive sil-
6 8 12 16 20 ica, portlandite reacted with dissolved carbon dioxide for giving
7 24.03 26.02 25.80 30.64 28.02 way to calcium carbonate. However, a part of portlandite com-
14 25.94 25.62 23.75 26.87 25.56 bined with alumina of metakaolin to form CAH10.
21 24.37 25.31 25.24 26.36 26.50
28 23.25 22.91 22.62 24 19.69
4. Conclusions

Thermally activated raw clay, essentially consisting of metaka-

As can be deduced from Table 4, water absorption laid in the olin, micaceous species and quartz, reacted with lime in humid
range 20–30%. It slightly changed with ageing time and increased environment to form C–S–H and CAH10 as well calcite. It appears
with the increase of lime content. It is believed that a major quan- that the occurrence of the former cementitious product required
tity of absorbed water was due to samples porosity and a residual small lime amounts and implicated particularly micaceous species
part, observed particularly for lime rich mixes, was due to hydra- and quartz. However, the formation of the later one implied
tion of calcite and portlandite. Referring to the kinetics curves of metakaolin and quantitative amounts of lime. Under the operating
Fig. 9, water absorption was a rapid process since samples satura- conditions, calcite formed as a result of the carbonation reaction,
tion was reached in less than 20 min. The mathematical treatment and unreacted portlandite was found, especially in lime rich mixes.
of the kinetics data showed that the variation of water absorption The formation of the cementitious compounds resulted in the
against time (t) obeyed the equation: Ln (1 Qt/Qe) = kt, where Qt increase of the bending strength. On the other hand, changes of

40 2; 6; 8; 12 ; 16 wt.% lime
mass of absorbed water/ mass of dried sample

30

20

10

0
0 20 40 60
Time (min)

Fig. 9. Kinetics curves relevant to the water absorption by thermally activated clay-lime mixes cured for different times.

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 Y. Mleza, M. Hajjaji / Construction and Building Materials xxx (2011) xxx–xxx
lime content and ageing time, and the resulting modification of
microstructure, had mitigated impacts on density and water
absorption.
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